Phosphorus oxychloride → HCID 131730134、化合物

反応式

[CH:1]([N:4]1[CH2:9][CH2:8][CH:7]([C:10]2[CH:11]=[CH:12][C:13](=O)[NH:14][N:15]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].O=P(Cl)(Cl)[Cl:19]>>[ClH:19].[Cl:19][C:13]1[N:14]=[N:15][C:10]([CH:7]2[CH2:8][CH2:9][N:4]([CH:1]([CH3:3])[CH3:2])[CH2:5][CH2:6]2)=[CH:11][CH:12]=1

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 68495857HCID 68495857、化合物

生成物 1

HCID 131730134HCID 131730134、化合物収率 88%

反応条件

温度: 60 °C

実験手順

6-(1-Isopropylpiperidin-4-yl)pyridazin-3-on (5.76 g, 26 mmol) was added to POCl3 (50 mL) and the reaction mixture was heated for 2 hours at 60° C. The excess of POCl3 was evaporated in vacuo and ethanol (96%) was added under an exothermic reaction. The reaction mixture was cooled and a precipitate was obtained. The product was filtered off after drying in vacuo and 6.34 g (88%) white crystals were isolated.

後処理

customThe excess of POCl3 was evaporated in vacuo and ethanol (96%)
additionwas added under an exothermic reaction
temperatureThe reaction mixture was cooled
customa precipitate was obtained
filtrationThe product was filtered off
customafter drying in vacuo

出典と根拠

ORDレコード: ord-d7730c9bd61244dda556684e9c298ef3
出典データセット: uspto-grants-2013_01
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08344001B2

反応ノート

読み込み中…

参加物